CN104371076B - A kind of method of normal temperature synthesis polycarboxylate water-reducer - Google Patents
A kind of method of normal temperature synthesis polycarboxylate water-reducer Download PDFInfo
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- CN104371076B CN104371076B CN201410726526.8A CN201410726526A CN104371076B CN 104371076 B CN104371076 B CN 104371076B CN 201410726526 A CN201410726526 A CN 201410726526A CN 104371076 B CN104371076 B CN 104371076B
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 18
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 16
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 15
- 239000007800 oxidant agent Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 150000008065 acid anhydrides Chemical class 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000002360 preparation method Methods 0.000 claims abstract 2
- 239000000178 monomer Substances 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical compound CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- 150000008064 anhydrides Chemical class 0.000 claims description 3
- XEEYSDHEOQHCDA-UHFFFAOYSA-N 2-methylprop-2-ene-1-sulfonic acid Chemical compound CC(=C)CS(O)(=O)=O XEEYSDHEOQHCDA-UHFFFAOYSA-N 0.000 claims description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical class OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 229930003268 Vitamin C Natural products 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 235000015424 sodium Nutrition 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- 235000019154 vitamin C Nutrition 0.000 claims description 2
- 239000011718 vitamin C Substances 0.000 claims description 2
- 239000012986 chain transfer agent Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 238000010526 radical polymerization reaction Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 239000004568 cement Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 208000014903 transposition of the great arteries Diseases 0.000 description 3
- 229930003231 vitamin Natural products 0.000 description 3
- 239000011782 vitamin Substances 0.000 description 3
- 235000013343 vitamin Nutrition 0.000 description 3
- 229940088594 vitamin Drugs 0.000 description 3
- 150000003722 vitamin derivatives Chemical class 0.000 description 3
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000002411 thermogravimetry Methods 0.000 description 2
- 238000012032 thrombin generation assay Methods 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000005395 methacrylic acid group Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- -1 polyoxy Polymers 0.000 description 1
- ASUAYTHWZCLXAN-UHFFFAOYSA-N prenol Chemical compound CC(C)=CCO ASUAYTHWZCLXAN-UHFFFAOYSA-N 0.000 description 1
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- Polymerization Catalysts (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a kind of method of normal temperature synthesis polycarboxylate water-reducer, preparation method comprises the following steps:1) under normal temperature, unsaturated APEO and water are added into reactor stirring；2) while A liquid and B liquid is added dropwise, A liquid is unsaturated carboxylic acid or acid anhydrides, the mixed aqueous solution of reducing agent and chain-transferring agent, and time for adding is 3 3.5h, and B liquid is aqueous oxidizing agent solution, and time for adding is 2 2.5h；3) curing 1h is dripped, adds sodium hydroxide solution, adjustment pH value to 57.The polycarboxylate water-reducer of the present invention is obtained using water as solvent by radical polymerization at normal temperatures.Whole building-up process saves the energy, reduces pollution, and water-reducing property is better than domestic and international product, can widely apply in the industrial production without heating.
Description
Technical field
The present invention relates to a kind of method of normal temperature synthesis polycarboxylate water-reducer, belong to technical field of concrete additives.
Background technology
In construction material, concrete is that dosage is maximum and most widely used, and as the poly- of concrete BSA
The advantages that carboxylic acid high-performance water reducing agent is because its dispersive property is good, water-reducing rate height, and plasticity is good is paid close attention to by academia, and near
Promoted rapidly in year a bit, applied to the Important Project such as railway, highway, bridge, tunnel, water power, harbour, airport, harbour, civilian
In.
With the continuous consumption of non-renewable energy resources, the earth will face lack of energy.Usual poly carboxylic acid series water reducer
Synthesis, which needs to be heated at high temperature, can just obtain, complex process, while the requirement to consersion unit is also high, how to reduce polycarboxylic-acid and subtracts
Energy resource consumption in aqua synthesis turns into the major issue that polycarboxylic acids synthesis faces.
The content of the invention
The technical problem to be solved in the present invention is, there is provided one kind synthesizes high performance polycarboxylate water-reducer at normal temperatures
Method, reduce energy resource consumption, improve active constituent content, and it is applied to industrial production.
The present invention solve the technical scheme that uses of its technical problem for：
A kind of method of normal temperature synthesis polycarboxylate water-reducer, its raw material include the component of following mass fraction：Unsaturation is poly-
100 parts of oxygen vinethene polymeric monomer, unsaturated carboxylic acid or anhydrides monomer 5-18 parts, oxidant 0.5-3 parts, reducing agent 0.01-0.3
Part, chain-transferring agent 0.05-0.8 parts, sodium hydroxide 1-5 parts.
Further, it comprises the following steps：
Step 1）At 25 DEG C -35 DEG C, by unsaturated APEO polymeric monomer and water with mass ratio 1：3 add reaction
Kettle, stirred with 85-95r/min；
A liquid and B liquid is added dropwise while stirring in step 2), and A liquid is the unsaturated carboxylic acid or acid anhydrides, reducing agent and chain
The mixed aqueous solution of transfer agent, time for adding 3-3.5h, 30-50mL being uniformly added dropwise per hour, B liquid is aqueous oxidizing agent solution,
Time for adding is 2-2.5h, and 20-30mL is uniformly added dropwise per hour；
Step 3) drips, and cures 1h, adds sodium hydroxide solution, adjustment pH value to 5-7.
Preferably, the unsaturated APEO polymeric monomer is methyl allyl polyoxyethylene ether or prenol polyoxy
Vinethene.
Preferably, the unsaturated APEO polymeric monomer degree of unsaturation is more than 0.37, weight average molecular weight 2400.
Preferably, the unsaturated carboxylic acid or acid anhydrides are at least one of acrylic acid, methacrylic acid or maleic anhydride.
Preferably, the oxidant be potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate, hydrogen peroxide or permanganic acid in extremely
Few one kind.
Preferably, the reducing agent be vitamin C, ferrous sulfate, sodium hypophosphite, oxalic acid or sodium thiosulfate in extremely
Few one kind.
Preferably, the chain-transferring agent is TGA, 2 mercaptopropionic acid, 3- mercaptopropionic acids or methallylsulfonic acid sodium
At least one of.
Preferably, the sodium hydroxide solution use mass concentration for 40% sodium hydrate aqueous solution.
The present invention is beneficial to be had the technical effect that：Present invention synthesis polycarboxylate water-reducer uses dropwise addition mode, big single before dropwise addition
Body need not all dissolve, and dissolved when being added dropwise, save the dissolution time of monomer, save the material time；Using being synthesized under normal temperature,
Whole building-up process saves the energy, no noxious emission, does not pollute the environment, can be widely used in industrial production without heating.
The polycarboxylate water-reducer water-reducing rate of this method synthesis is high, hence it is evident that better than like product.
Embodiment
In order that the technological means and operating process of the present invention are simple and clear, done further with reference to specific embodiment
Illustrate.
Embodiment 1：
The methyl allyl polyoxyethylene ether 360g and 270g of molecular weight 2400 water are added in four-hole bottle and stirred
20min.39g acrylic acid, 1.31g TGAs and 0.54g vitamin Cs are dissolved in 86g water, it is well mixed to obtain A liquid.Will
4.88g hydrogen peroxide and 52g water is mixed to get B liquid.A liquid and B liquid is added dropwise simultaneously, wherein A drops add 3h, and B drops add 2h, are added dropwise
Process is without heating.After being added dropwise, 1h is cured, the sodium hydroxide solution of 13g mass fractions 40% is added afterwards, adds running water
All solutes are adjusted in solution relative to the mass concentration of water to 40%, that is, obtain the poly carboxylic acid series water reducer of embodiment 1.
Embodiment 2：
The methyl allyl polyoxyethylene ether 360g and 270g of molecular weight 2400 water are added in four-hole bottle and stirred
20min.42g methacrylic acids, 1.40g TGAs and 0.60g vitamin Cs are dissolved in 86g water, it is well mixed to obtain A
Liquid.5.04g hydrogen peroxide and 52g water are mixed to get B liquid.A liquid and B liquid is added dropwise simultaneously, wherein A drops add 3.5h, and B drops add
2h, process is added dropwise without heating.After being added dropwise, 1h is cured, the sodium hydroxide solution of 14g mass fractions 40% is added afterwards, adds
In running water adjustment solution all solutes obtain poly carboxylic acid series water reducer of the invention relative to the mass concentration of water to 40%.
Embodiment 3：
The isoamyl alcohol polyoxyethylene ether 360g and 270g of molecular weight 2400 water are added in four-hole bottle and stir 20min.
43g acrylic acid, 1.59g mercaptopropionic acids and 0.66g vitamin Cs are dissolved in 86g water, it is well mixed to obtain A liquid.By 4.92g
Hydrogen peroxide and 52g water be mixed to get B liquid.A liquid and B liquid is added dropwise simultaneously, wherein A drops add 3h, and B drops add 2.5h, were added dropwise
Cheng Wuxu is heated.After being added dropwise, 1h is cured, the sodium hydroxide solution of 14g mass fractions 40% is added afterwards, adds running water to adjust
In whole solution all solutes obtain poly carboxylic acid series water reducer mother liquor of the invention relative to the mass concentration of water to 40%.
Embodiment 4-12
Embodiment 4-12 is to select component and parts by weight such as table 1 to match with embodiment difference.
The embodiment 4-12 of table 1 component and proportioning
The present invention also can be selected can in the unsaturated carboxylic acid or anhydrides monomer, oxidant, reducing agent and chain-transferring agent
Any independent assortment of component is selected, gross mass number meets present invention limitation.
Obtained water reducer in above-described embodiment 1-3 and the water reducer of comparative example 1 and 2 are subjected to performance comparison, experiment uses
The prosperous cement of P.O42.5 ancient cooking vessels and P.O42.5 Jis east cement carry out net slurry detection to obtained water reducer, and detection method is referring to GB-
8077-2010, specific net slurry flow-data are shown in Table 2.
Comparative example 1 is identical with the raw material of embodiment 1, the difference is that only that while stirring, A liquid and B is added dropwise in step 2)
Liquid, A liquid is the unsaturated carboxylic acid or acid anhydrides, the mixed aqueous solution of reducing agent and chain-transferring agent, time for adding 1h, per hour
100mL is uniformly added dropwise, B liquid is aqueous oxidizing agent solution, time for adding 0.5h, 100mL is uniformly added dropwise per hour.
Comparative example 2 is identical with the raw material of embodiment 2, the difference is that only that while stirring, A liquid and B is added dropwise in step 2)
Liquid, A liquid is the unsaturated carboxylic acid or acid anhydrides, the mixed aqueous solution of reducing agent and chain-transferring agent, time for adding 1h, per hour
100mL is uniformly added dropwise, B liquid is aqueous oxidizing agent solution, time for adding 0.5h, 100mL is uniformly added dropwise per hour.
The flowing degree of net paste of cement of table 2
Find out from the flowing degree of net paste of cement experimental result of table 2, the diminishing effect of polycarboxylate water-reducer prepared by 3 example normal temperature
Fruit is preferable, can carry out industrialized production and application.
The present invention is not limited to the above embodiments, simply illustrates the present invention described in above-described embodiment and specification
Principle, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, and these change and changed
Enter all fall within the protetion scope of the claimed invention.
Claims (8)
- A kind of 1. method of normal temperature synthesis polycarboxylate water-reducer, it is characterised in that its raw material includes the component of following mass fraction： Unsaturated 100 parts of APEO polymeric monomer, unsaturated carboxylic acid or anhydrides monomer 5-18 parts, oxidant 0.5-3 parts, reducing agent 0.01-0.3 parts, chain-transferring agent 0.05-0.8 parts, sodium hydroxide 1-5 parts；Preparation technology specifically comprises the following steps：Step 1）At 25 DEG C -35 DEG C, by unsaturated APEO polymeric monomer and water with mass ratio 1：3 add reactor, stir Mix；A liquid and B liquid is added dropwise while stirring in step 2), and A liquid is the unsaturated carboxylic acid or acid anhydrides, reducing agent and chain tra nsfer The mixed aqueous solution of agent, time for adding 3-3.5h, 30-50mL is uniformly added dropwise per hour, B liquid is aqueous oxidizing agent solution, is added dropwise Time is 2-2.5h, and 20-30mL is uniformly added dropwise per hour；Step 3) drips, and cures 1h, adds sodium hydroxide solution, adjustment pH value to 5-7.
- A kind of 2. method of normal temperature synthesis polycarboxylate water-reducer according to claim 1, it is characterised in that the unsaturation APEO polymeric monomer is methyl alkenyl APEO or isoamyl alcohol polyoxyethylene ether.
- A kind of 3. method of normal temperature synthesis polycarboxylate water-reducer according to claim 2, it is characterised in that the unsaturation APEO polymeric monomer degree of unsaturation is more than 0.37, weight average molecular weight 2400.
- A kind of 4. method of normal temperature synthesis polycarboxylate water-reducer according to claim 1, it is characterised in that the unsaturation Carboxylic acid or acid anhydrides are at least one of acrylic acid, methacrylic acid or maleic anhydride.
- A kind of 5. method of normal temperature synthesis polycarboxylate water-reducer according to claim 1, it is characterised in that the oxidant For at least one of potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate, hydrogen peroxide or permanganic acid.
- A kind of 6. method of normal temperature synthesis polycarboxylate water-reducer according to claim 1, it is characterised in that the reducing agent For at least one of vitamin C, ferrous sulfate, sodium hypophosphite, oxalic acid or sodium thiosulfate.
- A kind of 7. method of normal temperature synthesis polycarboxylate water-reducer according to claim 1, it is characterised in that the chain tra nsfer Agent is at least one of TGA, 2 mercaptopropionic acid, 3- mercaptopropionic acids or methallylsulfonic acid sodium.
- A kind of 8. method of normal temperature synthesis polycarboxylate water-reducer according to claim 1, it is characterised in that the hydroxide Sodium solution use mass concentration for 40% sodium hydrate aqueous solution.
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| CN113402194A (en) * | 2021-07-26 | 2021-09-17 | 中铁十一局集团桥梁有限公司 | Water reducing agent, preparation method thereof and concrete |
| CN114105513B (en) * | 2021-11-22 | 2022-10-25 | 云南森博混凝土外加剂有限公司 | Alkali-free accelerator and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286134A (en) * | 2011-06-09 | 2011-12-21 | 江苏天音化工有限公司 | Preparation method for high-performance water reducing agent |
| CN103172291A (en) * | 2012-12-14 | 2013-06-26 | 上海东大化学有限公司 | Polycarboxylic-acid water reducing agent synthesized at normal temperature, and preparation method and application method thereof |
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| CN102286134A (en) * | 2011-06-09 | 2011-12-21 | 江苏天音化工有限公司 | Preparation method for high-performance water reducing agent |
| CN103172291A (en) * | 2012-12-14 | 2013-06-26 | 上海东大化学有限公司 | Polycarboxylic-acid water reducing agent synthesized at normal temperature, and preparation method and application method thereof |
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